関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| 反応物 | 1,3-Benzodioxole-5-carboxylic acid | HCID 7196 | — |
| 反応物 | 2,3-Dimethylcyclohexylamine | HCID 123507 | — |
| 反応物 | Carbodiimide | HCID 160435 | — |
| 反応物 | HCID 178418300 | HCID 178418300 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Acetonitrile methylene chloride | HCID 21877088 | — |
| 生成物 | N-(2,3-dimethylcyclohexyl)benzo[d][1,3]dioxole-5-carboxamide | HCID 17479454 | — |
反応手順
2,3-dimethylcyclohexanamine (20 μmol) and benzo[d][1,3]dioxole-5-carboxylic acid (1.1 eq) were each dissolved in acetonitrile/dichloromethane (200 μL, 2:1). PS-Carbodiimide resin (2 eq) was loaded into a 1.2 mL 96 well Greiner plate, followed by the addition of amine and acid solutions. Hydroxybenzotriazole (1.1 eq) was dissolved in DMF (100 mL) and was added into the reaction well. The reaction was shaken overnight at room temperature. Once the reaction was completed, PS-Trisamine resin (1.5 eq) was added into the reaction mixture and the solution was allowed to shake overnight at room temperature. Acetonitrile (200 mL) was added into the reaction well, and the top clear solution was transferred into a new plate. The solution was evaporated to give N-(2,3-dimethylcyclohexyl)benzo[d][1,3]dioxole-5-carboxamide. MS (M+H, 276.20).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07476399B2 |
|---|
| 出典データセット | uspto-grants-2009_01 |
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| ORD ID | ord-ac0abaa13bb24876b7887cb3ae4727fc |
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| 出典メモ | uspto-grants-2009_01 |
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